JP4736222B2 - Method for producing magnesium alloy - Google Patents
Method for producing magnesium alloy Download PDFInfo
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- JP4736222B2 JP4736222B2 JP2001111726A JP2001111726A JP4736222B2 JP 4736222 B2 JP4736222 B2 JP 4736222B2 JP 2001111726 A JP2001111726 A JP 2001111726A JP 2001111726 A JP2001111726 A JP 2001111726A JP 4736222 B2 JP4736222 B2 JP 4736222B2
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Description
【０００１】
【発明の属する技術分野】
本発明は、マグネシウム合金の製造方法に関し、特に、鋳造組織を細粒化できると同時に高温強度を向上できるマグネシウム合金の製造方法に関する。
【０００２】
【従来の技術】
マグネシウム合金の鋳造組織の細粒化は、合金の機械的性質を向上させる上で極めて重要である。
従来から、マグネシウム合金の鋳造組織細粒化の一般的な方法として、ヘキサクロロエタン（Ｃ2Ｃｌ6）をマグネシウム合金溶湯に添加する方法が知られている。しかし、この方法はヘキサクロロエタンが高温のマグネシウム合金溶湯と接触した際に、塩素化炭化水素（ＣＨＣ）が発生して環境汚染源となるという問題がある。
【０００３】
特開2000-104136号公報には、環境汚染物質を発生しないマグネシウム合金の細粒化方法として、ＢおよびＭｎをマグネシウム合金溶湯に添加する技術が提案されている。しかしこの方法では、マグネシウム合金溶湯中へのＭｎの添加がＡｌ-Ｍｎ合金の形でしかできず、不要なＡｌ成分の存在によってマグネシウム合金の延性が低下する等の問題があった。
【０００４】
【発明が解決しようとする課題】
本発明は、環境汚染物質を発生させず、マグネシウム合金の延性を良好に維持しつつ、鋳造組織を細粒化できると同時に高温強度を向上できるマグネシウム合金の製造方法を提供することを目的とする。
【０００５】
【課題を解決するための手段】
上記の目的を達成するために、本発明のマグネシウム合金の製造方法は、粉末粒子の表面にＳｉＯ2被膜を備えたＳｉＣ粉末を、０．１〜１０mass％の添加量でマグネシウム合金溶湯に直接添加することを特徴とする。
ＳｉＣ粉末を大気中で加熱することにより粉末粒径の１〜１０％の厚さの前記ＳｉＯ2被膜を形成することが望ましい。
【０００６】
【発明の実施の形態】
粉末粒子の表面をＳｉＯ2で被覆したＳｉＣ粉末（以下「ＳｉＯ2被覆ＳｉＣ粉末」と略称する）をマグネシウム合金溶湯に添加することにより、マグネシウム合金の鋳造組織が細粒化すると同時に高温強度が向上する機構は以下のように考えられる。
【０００７】
Ｍｇ合金溶湯にＳｉＯ2被覆ＳｉＣ粉末を添加すると、まず粉末粒子表面のＳｉＯ2とＭｇが下記(1)の発熱反応をする。
その結果、粉末粒子表面が８５０℃以上の高温になるため、ＭｇとＳｉＣが下記(2)のように反応することが可能になり、Ｍｇ2Ｓｉ金属間化合物と遊離Ｃとが生成する。ここで生成したＭｇ2Ｓｉ金属間化合物により高温強度が向上する。
【０００８】
一方、遊離Ｃは、下記(3)のように、Ｍｇ合金中に一般的に含まれているＡｌ、Ｍｎ等の炭化物形成元素と反応してＡｌ4Ｃ3、Ｍｎ2Ｃ等の微細な金属炭化物粒子を形成する。これらの金属炭化物はＭｇ合金溶湯中で安定であり、凝固殻として作用するためＭｇ合金の鋳造組織が細粒化する。
【０００９】
(1) ２Ｍｇ＋ＳｉＯ2→２ＭｇＯ＋Ｓｉ （発熱反応）
(2) ２Ｍｇ＋ＳｉＣ→Ｍｇ2Ｓｉ＋Ｃ
(3) ３Ｃ＋４Ａｌ(またはＭｎ等）→Ａｌ4Ｃ3（またはＭｎ2Ｃ等）
【００１０】
本発明においては、ＳｉＯ2被覆ＳｉＣ粉末をＭｇ合金溶湯に対して０．１〜１０mass％の添加量で添加する。０．１mass％未満では細粒化効果が得られず、１０mass％を超えるとＭｇ合金溶湯の粘性が高くなり過ぎて鋳造が不可能になる。
【００１１】
本発明の望ましい態様においては、ＳｉＯ2被覆の厚さはＳｉＣ粒径の１〜１０％である。１％未満では、ＭｇとＳｉＯ2との反応による発熱量が少ないためＭｇとＳｉＣとの反応が起き難く、１０％を超えるとＭｇとＳｉＯ2とがテルミット反応を起こし易くなるため、Ｍｇ合金溶湯が爆発する危険がある。
【００１２】
【実施例】
下記の手順および条件により、ＳｉＯ2被覆ＳｉＣ粉末をＡＺ９１Ｄマグネシウム合金溶湯に直接添加した後に鋳造することにより、マグネシウム合金を製造した。
【００１３】
〔ＳｉＯ2被膜の形成〕
粉末粒径１０μｍのＳｉＣ粉末を大気中で加熱することにより、粉末粒子表面にＳｉＯ2被膜を形成した。まず加熱温度および加熱時間に対する被膜厚さの変化を調べた。図１および図２に、それぞれ加熱温度および加熱時間に対する被膜厚さの変化をグラフおよび表で示す。同様の予備実験を種々行い、それらの結果に基づいて、粒径の１〜１０％の被膜厚さになる温度・時間の範囲を求めた。
【００１４】
本実施例では、１５００℃×１時間の加熱を行い、ＳｉＣ粉末粒子の表面に厚さ４１１ｎｍのＳｉＯ2被膜を形成した。この被膜厚さは、ＳｉＣ粒径１００００ｎｍ（＝１０μｍ）の４．１％である。
加熱前および加熱後の粉末についてＸ線回折を行った結果、加熱前にはＳｉＣの回折ピークのみが認められたのに対して、加熱後にはＳｉＣピークに加えてＳｉＯ2の回折ピークが明瞭に認められた。これにより、被膜組成がＳｉＯ2であることが確認された。
【００１５】
〔マグネシウム合金溶湯への添加〕
ＳＦ6ガス雰囲気中にて、７００℃に保持したＡＺ９１Ｄマグネシウム合金溶湯に、上記にて準備したＳｉＯ2被覆ＳｉＣ粉末を種々の添加量で添加し、攪拌して溶湯中に均一に分散させた後、金型（ＪＩＳ４号舟型）中に鋳造した。
【００１６】
〔結晶粒径の測定〕
上記鋳造されたマグネシウム合金の鋳造組織を顕微鏡観察して結晶粒径を求めた。図３に、典型的な観察例として、ＳｉＯ2被覆ＳｉＣ粉末を１mass％添加した場合の鋳造組織を示す。図４に、比較として、無添加の場合の鋳造組織を示す。図５に、ＳｉＯ2被覆ＳｉＣ粉末の添加量と結晶粒径との関係をグラフおよび表で示す。
【００１７】
図５に示したように、ＳｉＯ2被覆ＳｉＣ粉末の添加量が０〜０．０５mass％の範囲では結晶粒径が２００〜１８０μｍと粗大であるが、添加量が０．１mass％以上になると８０〜５０μｍと顕著に細粒化する。同図には、添加量０．５mass％までの結果を示したが、添加量が更に多くなっても細粒化の程度は徐々に進行するが顕著に進行することはない。
【００１８】
〔高温強度の測定〕
(1)高温硬さの測定
上記鋳造されたマグネシウム合金の１５０℃における高温硬さを測定した。図６にＳｉＯ2被覆ＳｉＣ粉末の添加量と高温硬さとの関係をグラフおよび表で示す。
図６に示したように、１５０℃高温硬さはＳｉＯ2被覆ＳｉＣ粉末の添加量の増加に伴い単調に増加する。特に、図示した添加量４mass％までの範囲では、マグネシウム合金マトリクス中の硬質分散相であるＳｉＯ2被覆ＳｉＣ粉末の添加量に対して、硬さが概ね直線関係にあることが観察される。
【００１９】
このようにＳｉＯ2被覆ＳｉＣ粉末の添加によって高温硬さが増加するのは、基本的には前述のようにＭｇ2Ｓｉ金属間化合物が生成していることによる。図７に、ＳｉＯ2被覆ＳｉＣ粉末を１mass％添加したマグネシウム合金鋳造組織の顕微鏡写真を示す。同図中で、地の色と同等の灰色に見える塊状の粒子は、ＭｇＳｉ金属間化合物を核に形成されたと考えらるＭｇ-Ｓｉ-Ａｌ-Ｏ系４元化合物であり、Ｍｇ2Ｓｉ金属間化合物と同様に高温強度の向上に寄与する。
【００２０】
(2)高温軸力保持率の測定
ＳｉＯ2被覆ＳｉＣ粉末を１mass％添加したマグネシウム合金について、初期荷重６４ＭＰａ、試験温度１５０℃にて、負荷開始からの経過時間に対して軸力保持率を測定した。比較として、無添加のマグネシウム合金についても同様に測定した。図８に測定結果をグラフおよび表で示す。
【００２１】
図８に示したように、軸力保持率は時間経過に伴って低下し、無添加の比較例の場合には１００時間経過した時点で軸力保持率が０になった。これに対して、本発明によりＳｉＯ2被覆ＳｉＣ粉末を１mass％添加した場合には、１００時間経過した時点では軸力保持率はまだ２０％を維持しており、０にまで低下するのに経過時間３００時間を要した。このようにＳｉＯ2被覆ＳｉＣ粉末の添加により軸力保持特性が大幅に向上する。
【００２２】
【発明の効果】
以上説明したように、本発明により、環境汚染物質を発生させず、マグネシウム合金の延性を良好に維持しつつ、鋳造組織を細粒化できると同時に高温強度を向上できるマグネシウム合金の製造方法が提供される。
【図面の簡単な説明】
【図１】図１は、ＳｉＣ粉末の加熱温度と、粉末粒子表面に形成されたＳｉＯ2被膜の厚さとの関係を示すグラフおよび表である。
【図２】図２は、ＳｉＣ粉末の加熱時間と、粉末粒子表面に形成されたＳｉＯ2被膜の厚さとの関係を示すグラフおよび表である。
【図３】図３は、本発明によりＳｉＯ2被覆ＳｉＣ粉末を添加して製造したマグネシウム合金の鋳造組織を示す顕微鏡写真である。
【図４】図４は、比較例として無添加で製造したマグネシウム合金の鋳造組織を示す顕微鏡写真である。
【図５】図５は、ＳｉＯ2被覆ＳｉＣ粉末の添加量とマグネシウム合金の結晶粒径との関係を示すグラフおよび表である。
【図６】図６は、ＳｉＯ2被覆ＳｉＣ粉末の添加量と高温硬さとの関係を示すグラフおよび表である。
【図７】図７は、本発明によりＳｉＯ2被覆ＳｉＣ粉末を添加して製造したマグネシウム合金の鋳造組織中の析出化合物を示す顕微鏡写真である。
【図８】図８は、本発明によりＳｉＯ2被覆ＳｉＣ粉末を添加して製造したマグネシウム合金と、比較例として無添加で製造したマグネシウム合金とについて、高温での軸力保持率を時間経過に対して示すグラフおよび表である。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method for producing a magnesium alloy, and more particularly to a method for producing a magnesium alloy that can refine a cast structure and improve high-temperature strength at the same time.
[0002]
[Prior art]
Refinement of the cast structure of magnesium alloy is extremely important in improving the mechanical properties of the alloy.
Conventionally, a method of adding hexachloroethane (C 2 Cl 6 ) to a molten magnesium alloy is known as a general method for refining a cast alloy of a magnesium alloy. However, this method has a problem that chlorinated hydrocarbons (CHC) are generated when hexachloroethane comes into contact with the molten magnesium alloy at a high temperature and become a source of environmental pollution.
[0003]
Japanese Patent Application Laid-Open No. 2000-104136 proposes a technique of adding B and Mn to a molten magnesium alloy as a method for refining a magnesium alloy that does not generate environmental pollutants. However, this method has a problem that the addition of Mn into the molten magnesium alloy can be performed only in the form of an Al—Mn alloy, and the ductility of the magnesium alloy is lowered due to the presence of an unnecessary Al component.
[0004]
[Problems to be solved by the invention]
An object of the present invention is to provide a method for producing a magnesium alloy capable of reducing the cast structure and improving the high-temperature strength while maintaining good ductility of the magnesium alloy without generating environmental pollutants. .
[0005]
[Means for Solving the Problems]
In order to achieve the above object, the method for producing a magnesium alloy according to the present invention directly adds SiC powder having a SiO 2 coating on the surface of powder particles to a molten magnesium alloy in an addition amount of 0.1 to 10 mass%. It is characterized by doing.
It is desirable to form the SiO 2 coating having a thickness of 1 to 10% of the powder particle size by heating SiC powder in the air.
[0006]
DETAILED DESCRIPTION OF THE INVENTION
By adding SiC powder coated with SiO 2 on the surface of the powder particles (hereinafter abbreviated as “SiO 2 coated SiC powder”) to the molten magnesium alloy, the cast structure of the magnesium alloy becomes finer and at the same time the high-temperature strength is improved. The mechanism to perform is considered as follows.
[0007]
When SiO 2 -coated SiC powder is added to the molten Mg alloy, first, SiO 2 and Mg on the surface of the powder particles undergo an exothermic reaction (1) below.
As a result, the powder particle surface becomes a high temperature of 850 ° C. or higher, so that Mg and SiC can react as shown in (2) below, and an Mg 2 Si intermetallic compound and free C are generated. The high temperature strength is improved by the Mg 2 Si intermetallic compound produced here.
[0008]
On the other hand, free C reacts with carbide-forming elements such as Al and Mn that are generally contained in Mg alloys as shown in (3) below, so that fine metals such as Al 4 C 3 and Mn 2 C can be obtained. Form carbide particles. Since these metal carbides are stable in the molten Mg alloy and act as a solidified shell, the cast structure of the Mg alloy becomes finer.
[0009]
(1) 2Mg + SiO 2 → 2MgO + Si (exothermic reaction)
(2) 2Mg + SiC → Mg 2 Si + C
(3) 3C + 4Al (or Mn etc.) → Al 4 C 3 (or Mn 2 C etc.)
[0010]
In the present invention, the SiO 2 -coated SiC powder is added in an amount of 0.1 to 10 mass% with respect to the molten Mg alloy. If it is less than 0.1 mass%, the effect of refining cannot be obtained, and if it exceeds 10 mass%, the viscosity of the molten Mg alloy becomes so high that casting becomes impossible.
[0011]
In a preferred embodiment of the present invention, the thickness of the SiO 2 coating is 1-10% of SiC particle size. If it is less than 1%, the calorific value due to the reaction between Mg and SiO 2 is small, so that the reaction between Mg and SiC hardly occurs, and if it exceeds 10%, the thermite reaction easily occurs between Mg and SiO 2. There is a risk of explosion.
[0012]
【Example】
According to the following procedure and conditions, the SiO 2 coated SiC powder was directly added to the molten AZ91D magnesium alloy and then cast to produce a magnesium alloy.
[0013]
[Formation of SiO 2 coating]
By heating SiC powder having a powder particle size of 10 μm in the air, a SiO 2 coating was formed on the surface of the powder particles. First, changes in the film thickness with respect to the heating temperature and the heating time were examined. FIG. 1 and FIG. 2 are graphs and tables showing changes in film thickness with respect to heating temperature and heating time, respectively. Various similar preliminary experiments were conducted, and based on the results, a range of temperature and time at which the film thickness was 1 to 10% of the particle diameter was obtained.
[0014]
In this example, heating was performed at 1500 ° C. for 1 hour to form a 411 nm thick SiO 2 film on the surface of the SiC powder particles. This film thickness is 4.1% with a SiC particle size of 10000 nm (= 10 μm).
As a result of performing X-ray diffraction on the powder before heating and after heating, only the diffraction peak of SiC was observed before heating, whereas the diffraction peak of SiO 2 was clearly added in addition to the SiC peak after heating. Admitted. This confirmed that the coating composition was SiO 2 .
[0015]
[Addition to magnesium alloy melt]
After adding the SiO 2 -coated SiC powder prepared above in various addition amounts to the AZ91D magnesium alloy molten metal maintained at 700 ° C. in an SF 6 gas atmosphere, and stirring and uniformly dispersing in the molten metal , And cast into a mold (JIS No. 4 boat type).
[0016]
(Measurement of crystal grain size)
The crystal grain size was determined by microscopic observation of the cast structure of the cast magnesium alloy. FIG. 3 shows a cast structure in the case where 1 mass% of SiO 2 -coated SiC powder is added as a typical observation example. FIG. 4 shows a cast structure in the case of no addition as a comparison. FIG. 5 is a graph and a table showing the relationship between the addition amount of the SiO 2 -coated SiC powder and the crystal grain size.
[0017]
As shown in FIG. 5, when the addition amount of the SiO 2 -coated SiC powder is in the range of 0 to 0.05 mass%, the crystal grain size is as coarse as 200 to 180 μm, but when the addition amount is 0.1 mass% or more, it is 80 It is remarkably fined to ˜50 μm. Although the results up to the addition amount of 0.5 mass% are shown in the figure, the degree of atomization gradually progresses but does not progress significantly even if the addition amount is further increased.
[0018]
[Measurement of high-temperature strength]
(1) Measurement of high-temperature hardness The high-temperature hardness at 150 ° C of the cast magnesium alloy was measured. FIG. 6 is a graph and a table showing the relationship between the addition amount of the SiO 2 -coated SiC powder and the high temperature hardness.
As shown in FIG. 6, the 150 ° C. high temperature hardness increases monotonically with the increase in the amount of SiO 2 -coated SiC powder added. In particular, in the range up to the added amount of 4 mass% shown in the figure, it is observed that the hardness is generally linearly related to the added amount of the SiO 2 -coated SiC powder that is the hard dispersed phase in the magnesium alloy matrix.
[0019]
The reason why the high temperature hardness is increased by the addition of the SiO 2 coated SiC powder is basically due to the formation of the Mg 2 Si intermetallic compound as described above. FIG. 7 shows a micrograph of a magnesium alloy cast structure to which 1 mass% of SiO 2 -coated SiC powder is added. In the figure, the massive particles that appear gray like the ground color are Mg—Si—Al—O quaternary compounds that are thought to be formed with MgSi intermetallic compounds as nuclei, and Mg 2 Si metal. Like the intermetallic compound, it contributes to the improvement of high temperature strength.
[0020]
(2) Measurement of high-temperature axial force retention rate With respect to a magnesium alloy to which 1 mass% of SiO 2 -coated SiC powder was added, the axial force retention rate was measured with respect to the elapsed time from the start of load at an initial load of 64 MPa and a test temperature of 150 ° C. did. For comparison, the same measurement was performed for an additive-free magnesium alloy. FIG. 8 shows the measurement results in a graph and a table.
[0021]
As shown in FIG. 8, the axial force retention rate decreased with time, and in the case of the additive-free comparative example, the axial force retention rate became zero after 100 hours. On the other hand, when 1 mass% of SiO 2 -coated SiC powder is added according to the present invention, the axial force retention rate is still maintained at 20% when 100 hours have elapsed, and it has been reduced to zero. It took 300 hours. Thus, the axial force retention characteristics are greatly improved by the addition of the SiO 2 -coated SiC powder.
[0022]
【The invention's effect】
As described above, according to the present invention, there is provided a method for producing a magnesium alloy capable of reducing the cast structure and improving the high-temperature strength while maintaining good ductility of the magnesium alloy without generating environmental pollutants. Is done.
[Brief description of the drawings]
FIG. 1 is a graph and a table showing the relationship between the heating temperature of SiC powder and the thickness of a SiO 2 film formed on the surface of powder particles.
FIG. 2 is a graph and a table showing the relationship between the heating time of SiC powder and the thickness of the SiO 2 film formed on the surface of the powder particles.
FIG. 3 is a photomicrograph showing the cast structure of a magnesium alloy produced by adding SiO 2 coated SiC powder according to the present invention.
FIG. 4 is a photomicrograph showing the cast structure of a magnesium alloy produced as a comparative example without addition.
FIG. 5 is a graph and table showing the relationship between the addition amount of SiO 2 -coated SiC powder and the crystal grain size of the magnesium alloy.
FIG. 6 is a graph and table showing the relationship between the addition amount of SiO 2 -coated SiC powder and high-temperature hardness.
FIG. 7 is a photomicrograph showing a precipitated compound in a cast structure of a magnesium alloy produced by adding SiO 2 coated SiC powder according to the present invention.
FIG. 8 is a graph showing the axial force retention at high temperatures over time for a magnesium alloy produced by adding SiO 2 -coated SiC powder according to the present invention and a magnesium alloy produced without addition as a comparative example. It is the graph and table | surface shown with respect to it.
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001111726A JP4736222B2 (en) | 2001-04-10 | 2001-04-10 | Method for producing magnesium alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001111726A JP4736222B2 (en) | 2001-04-10 | 2001-04-10 | Method for producing magnesium alloy |
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| JP4736222B2 true JP4736222B2 (en) | 2011-07-27 |
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